NIST Procedure For Method Validation 20180101

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This procedure is a sample template provided to support training seminars and webinars and may be adopted by

laboratories as a good laboratory practice, good measurement practice, or administrative procedure.

Procedure for Method Validation

1. Introduction

This is the metrology laboratory policy and procedure for developing and validating test or
calibration methods when no international or national procedures are available, when
deviating from standardized methods, or when no standard procedures are available.

2. Purpose

The Metrology Laboratory follows this procedure to ensure that all laboratory methods selected,
modified, or developed for tests and calibrations are appropriate for the intended use, properly
documented, validated, accepted by laboratory management, and agreed upon by the client.
Customers of the Laboratory expect a given service to provide acceptable measurement results
when they request a test or calibration. The laboratory must evaluate each method to ensure that
it has qualified and competent staff, suitable facilities, equipment, and standards with acceptable
metrological traceability to perform the test or calibration.

3. Responsibility

3.1.The Laboratory Supervisor or Quality Manager ensures the following, in consultation


with the laboratory staff as needed:
3.1.1. Development of methods is a planned activity and assigned to qualified staff with
appropriate resources.
3.1.2. For larger projects, plans are updated as progress is made and effectively
communicated to all personnel.
3.1.3. Ensure the report for the test or calibration is compliant with standard
requirements and customer needs.

3.2. The Technical Manager reviews the documented procedure, data, and analysis, and
recommends final acceptance to the Laboratory Manager or Quality Manager based on
the suitability of the procedure and acceptability of observed analysis of measurement
results.

3.3. The Laboratory Supervisor or Quality Manager is responsible for final acceptance of
new calibration methods, training staff on the new procedure, and for consistent
implementation.

4. Operations

4.1.If the laboratory does not have an appropriate method for a calibration or test, or the test
or calibration requires deviation to meet the needs of the customer, the Technical
Manager is notified and this procedure is implemented.

4.2. When determining whether to proceed in developing new test or calibration method to
meet the needs of a customer, the Laboratory Supervisor or Quality Manager and

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Technical Manager consider at least the following factors:
4.2.1. Availability of alternative procedures (national or international standards);
4.2.2. Resources of the laboratory and staffing (time, efficiency); and
4.2.3. Likely future demand for the service.

4.3. The staff conducting the Contract Review for the calibration or test must obtain a clear
specification of the customer requirements and the purpose of the test or calibration
including any tolerances or maximum uncertainties that are required for the item/sample
end usage (to ensure that the measurement results will be fit for purpose).

4.4. New methods must be developed prior to performing the tests or calibrations and contain
the following information:
4.4.1. appropriate identification (title);
4.4.2. scope or range of test;
4.4.3. description of the type of item to be tested or calibrated;
4.4.4. parameters or quantities and ranges to be determined;
4.4.5. apparatus and equipment, including technical performance requirements;
4.4.6. reference standards and reference materials required;
4.4.7. environmental conditions required and any stabilization period needed;
4.4.8. description of the procedure, including any special items as noted in this list:
4.4.8.1. affixing of identification marks, handling, transporting, storing and
preparation of items,
4.4.8.2. checks to be made before the work is started,
4.4.8.3. checks that the equipment is working properly and, where required,
calibration and adjustment of the equipment before each use,
4.4.8.4. the method of recording the observations, data to be recorded, data
reduction, method of analysis, and presentation of results, and
4.4.8.5. any safety measures to be observed;
4.4.9. criteria and/or requirements for approval/rejection where applicable;
4.4.10. data to be recorded and method of analysis and presentation; and
4.4.11. the uncertainty or the procedure for estimating uncertainty.

5. Method Validation

5.1. Non-standardized methods, which include all laboratory developed methods,


standardized methods modified beyond their intended scope and amplifications and
modifications of standardized methods, are validated by:
5.1.1. Examination to ensure completeness and compliance with requirements for
essential components of metrological traceability; and
5.1.2. Analysis of objective evidence to ensure the requirements for a specific intended
purpose are fulfilled prior to use.

5.2. Validation methods are to be as extensive as necessary to meet the needs of their
intended application. Adequate measurement data is obtained to ensure statistical
validity of the evaluated results. The accuracy and uncertainty of test or calibration
results shall be assessed for the intended use, and shall be relevant to the client’s needs.

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5.3. Validation procedures and results are recorded, with a statement concerning the
appropriateness of the new method as it pertains to the intended use.

5.4. Validation techniques include one or a combination of the following:


5.4.1. Calibration/verification and evaluation of bias and precision using calibrated
working standards;
5.4.2. Comparison of results achieved with other standardized methods;
5.4.3. Method evaluation through variations of controlled parameters (e.g., one variable
at a time) to determine robustness;
5.4.4. Inter-laboratory comparisons when practical;
5.4.5. Systematic assessment of factors influencing the results; and
5.4.6. Evaluation of the uncertainty of results based on scientific understanding of the
theoretical principles associated with the method and practical experience.

5.5. When changes are made in the validated non-standardized procedures, the influence of
such changes must be documented and, if appropriate, a new validation process carried
out.

5.6. The following types of assessments, with data and statistical analysis are examples that
may be used to assess the measurement results (See Appendix A form):
5.6.1. Inspection and technical assessment of the essential elements of metrological
traceability to ensure presence and adequacy (technical review may include
representatives from other laboratories, working groups, technical experts, and
assessors):
5.6.1.1. Reference to the international system of units (SI);
5.6.1.2. Unbroken chain of calibrations to national and/or international standards;
5.6.1.3. Suitable and up to date calibration intervals for standards used in the
procedure;
5.6.1.4. Documented procedure (reviewed to ensure completeness against the list
of items in Section 4.d.);
5.6.1.5. Documented measurement uncertainty (as noted in Section 4.d.v.);
5.6.1.6. Demonstrated technical competence;
5.6.1.7. Adequate measurement assurance approach and supporting data.
5.6.2. Accuracy or Limits to Bias may use data obtained from internal testing and/or
interlaboratory comparisons: t-test, normalized error (En), absolute or relative bias
versus required tolerance limits;
5.6.3. Precision: standard deviation, normalized precision (Pn), F-test, comparison to
required uncertainties (fit for purpose and meeting needs of the customer)
5.6.4. Repeatability: assessment of results over time and by different operators
following the procedure as documented
5.6.5. Reproducibility: assessment of data from other laboratories following the
procedure

6. Records (See Appendix A for minimum summary to be supplemented with appropriate data,
analysis, and evaluation records).

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6.1. Laboratory records shall be retained for all aspects of the procedure validation for as
long as the procedure remains in valid use, including but not limited to:
6.1.1. The validation procedure (and version) that is used;
6.1.2. Any applicable specifications and/or tolerances;
6.1.3. Evaluation of performance characteristics and summaries;
6.1.4. Observed data and measurement results;
6.1.5. Approval for use by the customer; and
6.1.6. A statement that the method is valid and suitable for its intended use.

7. Implementation

7.1. A laboratory developed test or calibration method is validated, reviewed by the


Technical Manager, reviewed by the Quality Manager, and approved by the Laboratory
Supervisor.
7.2. A laboratory developed test or calibration method is validated, reviewed by the
Technical Manager, reviewed by the Quality Manager, and approved by the Laboratory
Supervisor.
7.3. The method is documented and formatted into a written Standard Operating Procedure
(SOP) document and assigned an identification number. The new SOP will be added to
the laboratory Master List.
7.4. Staff are trained and competency is confirmed.
7.5. All laboratory method validation documentation is kept on file in the laboratory and
maintained according to the Quality Management System.

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Appendix A
Evaluation Form for Method Validation Review

Procedure Evaluated: ____________________________________

Evaluation Conducted by: ____________________________________

Method Evaluation Observations


Procedure is complete and contains:
appropriate identification (title);
scope or range of test;
description of the type of item to be tested or calibrated;
parameters or quantities and ranges to be determined;
apparatus and equipment, including technical performance
requirements;
reference standards and reference materials required;
environmental conditions required and any stabilization period
needed;
description of the procedure, including any special items as
noted in this list:
affixing of identification marks, handling, transporting,
storing and preparation of items,
checks to be made before the work is started,
checks that the equipment is working properly and, where
required, calibration and adjustment of the equipment
before each use,
the method of recording the observations, data to be
recorded, data reduction, method of analysis, and
presentation of results, and
any safety measures to be observed;
criteria and/or requirements for approval/rejection where
applicable;
data to be recorded and method of analysis and presentation;
and
the uncertainty or the procedure for estimating uncertainty.
Essential Elements of Traceability are Defined (5.f, i) See GMP
13.
Realization of SI Units. The primary national, international, or
intrinsic standards must be primary standards for the realization of
the International System of Units (SI);
Unbroken chain of comparisons. A documented system of
comparisons with each step having the essential elements of
metrological traceability going back to a standard acceptable to the
parties, usually a national or international standard; Are suitable
standards identified in the procedure?

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Method Evaluation Observations
Standard Calibrations & Intervals. Calibrations of standards (and
equipment where appropriate) must be repeated at established
(may be defined through measurement assurance) and appropriate
intervals to preserve metrological traceability of the standard over
time and use (see GLP 4, GMP 11); Are suitable calibration
intervals defined for the standards used in this procedure?
Documented Measurement Uncertainty. The measurement
uncertainty for each step in the traceability chain must be
calculated according to defined methods and must be stated so that
an overall uncertainty for the whole chain may be calculated (see
SOP 29); Is the uncertainty budget completely defined based on a
comparison of similar procedures or technical reference
documents (describe the procedures and/or references)
Documented Measurement Procedure. Each step in the chain must
be performed according to documented and generally
acknowledged procedures (see GMP 12) and the results must be
documented (i.e., in a calibration certificate, see SOP 1); Is the
procedure complete according to all required elements?
(4.d)
Accredited Technical Competence. The laboratories or bodies
performing one or more steps in the chain must supply evidence of
technical competence (e.g., by maintaining appropriate training
records, participating in interlaboratory comparisons, and by
demonstrating that they are accredited by a recognized
accreditation body); Have all staff been trained and have they
demonstrated competency with the procedure? Have any other
laboratories provided input or tried to duplicate the procedure?
Was an interlaboratory comparison or proficiency test conducted?
Describe the results.
Measurement assurance. A proper measurement assurance
program must be established to ensure the validity of the
measurement process and the accuracy of standard used at the time
of the measurement (see SOPs 9, 17, 20, 30). What type of
measurement assurance is integrated into the procedure? Describe
what the measurement assurance monitors (standards, process,
both? How?)
Additional Assessments
Comparison of Results with Other Procedures. Describe what
other procedures or standards were considered and why/why not
chosen? Describe the results obtained and analysis conducted with
multiple procedures.
Evaluation of Accuracy and Bias. (5.f.ii)
What are the limits to bias or error? How do you know the results
are right? Describe the recently calibrated standard/set of
standards that were used. Describe any standard reference
materials that were used. How were the results assessed for
Accuracy?

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Method Evaluation Observations
Evaluation of Precision. How was data for repeatability obtained?
Describe whether the precision assessment is short-term or long-
term and if short-term, how do you know how the procedure will
repeat over time? How do you know whether the precision is
sufficiently small when incorporated into uncertainties? Describe
the statistical assessments that were completed and document the
analysis results.
Evaluation of Repeatability. E.g., two different units were
evaluated after a recent (enter dates) calibration by multiple
metrologists; what kind of statistics were used and what were the
results? (Consider repeatability with different staff, equipment,
standards/nominal values, and not just short-term precision.)
Evaluation of Reproducibility. Have any other laboratories
provided input or tried to duplicate the procedure? Was an
interlaboratory comparison or proficiency test conducted?
Describe the results.
3rd Party Assessment or Technical Reviews. Have any other
technical experts reviewed the procedure and provided input?
Describe their assessment and any recommended improvements or
changes that were implemented because of the review.

This procedure has found to be complete, fit for its intended use, technically validated, meets customer needs,
and is approved for use.

Quality Manager Signature Technical Manager Signature

Quality Manager Name (Printed) Technical Manager Name (Printed)

Date Date

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